CN106145959B - 一种氧化镥透明陶瓷的制备方法 - Google Patents

一种氧化镥透明陶瓷的制备方法 Download PDF

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CN106145959B
CN106145959B CN201610536089.2A CN201610536089A CN106145959B CN 106145959 B CN106145959 B CN 106145959B CN 201610536089 A CN201610536089 A CN 201610536089A CN 106145959 B CN106145959 B CN 106145959B
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luteium oxide
lutetium
crystalline ceramics
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王殿元
段兴凯
王庆凯
王侃民
郭艳艳
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Jiujiang University
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Abstract

本发明公开了一种氧化镥透明陶瓷的制备方法。该方法包括如下步骤：以水合硝酸镥和硫脲为原料，采用低温燃烧法制备获得纳米硫氧化镥(Lu2O2S)粉体；将所得硫氧化镥纳米粉体研磨、干压成型，于900‑1000℃空气烧结和1400‑1500℃真空烧结，得到氧化镥透明陶瓷。本发明的制备方法具有烧结温度低，成本低，易于操作等优点，制备出的氧化镥陶瓷致密度高、透光度好。

Description

一种氧化镥透明陶瓷的制备方法
技术领域
本发明涉及一种氧化镥透明陶瓷的制备方法，具体属于陶瓷材料制备技术领域。
背景技术
氧化镥Lu2O3是一种极有前途的激光与闪烁体基质材料，在可见光与红外光下均具有高透过率，其发射截面大，声子能量低，密度高，同时具有良好的机械性能与热性能。然而Lu2O3熔点高 达2450℃，采用提拉法生长含各种掺杂组分的单晶材料不仅工艺难实现，而且代价相当高。Lu2O3具有立方晶系结构，光学各向同性，折射率不依赖于方向性，可通过纳米晶技术和高温烧结技术将粉体制成透明陶瓷。因此研制氧化镥基透明陶瓷材料是这类材料获得应用的关键。而获得透明陶瓷材料的关键是先制备烧结性能优异的前驱粉体，要求粉体具有良好的分散性、粒径小、球形形貌等，低温燃烧法是达到这一目的的可行方法之一。
近年来，Lu2O3基透明陶瓷的研究已经得到了极大的关注。例如，A.Lempicki等人用草酸盐沉淀法合成Eu3+掺杂的Lu2O3陶瓷闪烁体，由于草酸盐Ksp较大，采用草酸盐沉淀法获得粉体颗粒尺寸较大，而且极易团聚；E.Zych等利用尿素作燃料用溶液燃烧法合成RE3+掺杂的Lu2O3发光粉体，然后真空烧结，仅能获得半透明的陶瓷样品，这是因为燃烧合成粉体团聚严重，烧结活性低；发明专利1510813014.X以氟化锂和氧化锆为烧结助剂，经成型和1850℃真空烧结得到Lu2O3基透明陶瓷，透过率超过80%，由于加入了烧结助剂，影响和降低了其发光性能；发明专利CN200510027208.3用沉淀法获得Lu2O3纳米粉体，然后经成型和1850℃真空烧结得到Lu2O3基透明陶瓷，所用烧结温度太高，成本较高。因此，发明一种新的Lu2O3基透明陶瓷材料的制备方法是非常有实际意义的。
发明内容
本发明的目的在于提供一种氧化镥透明陶瓷的制备方法，具体通过以下技术方案实现。
本发明公开了一种氧化镥透明陶瓷的制备方法，包括如下步骤：
将水合硝酸镥2.274g溶于50ml水中，得溶液A；将乙二醇5ml和硫脲1.37g分别加入到溶液A中，磁力搅拌，得均匀混合溶液B，将混合液B置于500℃马弗炉中，燃烧完毕后得到硫氧化镥纳米粉体；水合硝酸镥与硫脲摩尔比为1:3-4，乙二醇与水的体积比为1:10-15。
将步骤(1)所得的硫氧化镥粉体研磨30min，50Mpa双向轴压成型为陶瓷生胚片；将陶瓷生胚片于马弗炉中900-1000℃空气气氛下烧结10-15h，再于真空炉中1400-1500℃烧结2h，最后在马弗炉中900-1000℃空气气氛下退火5-6h，制得氧化镥透明陶瓷。
本发明的有益效果:本发明公开的氧化镥透明陶瓷的制备方法采用了自制的硫氧化镥Lu2O2S纳米粉作为陶瓷粉体原料，在1000℃马弗炉中烧结过程中，硫氧化镥被氧化成氧化镥Lu2O3，再将陶瓷胚片于1400-1500℃真空炉中高温烧结，可以进一步消除陶瓷片内的气孔，使颗粒长大，并提高陶瓷致密度，最后在900℃马弗炉中退火是为了消除真空烧结产生的氧空位，提高陶瓷透光度。该方法使用了三步烧结（退火）法，大大缩短了高温真空烧结的时间（通常高温真空烧结时间为6-10h），降低了成本，有利于氧化镥基透明陶瓷材料的（半）工业化生产。
附图说明
图1为本发明氧化镥透明陶瓷实物照片。
具体实施方式
实施例1
一种氧化镥透明陶瓷的制备方法，包括以下步骤：
将水合硝酸镥2.274g溶于50ml水中，得溶液A；将乙二醇5ml和硫脲1.37g分别加入到溶液A中，磁力搅拌，得均匀混合溶液B，将混合液B置于500℃马弗炉中，燃烧完毕后500℃退火1h,得到硫氧化镥Lu2O2S纳米粉体；
将步骤(1)所得的硫氧化镥粉体研磨30min，50Mpa双向轴压成型为陶瓷生胚片；将陶瓷生胚于马弗炉中1000℃空气气氛下烧结10h，再于真空炉中1400℃烧结2h，最后在马弗炉中900℃空气气氛下退火5h，制得氧化镥Lu2O3透明陶瓷。

Claims (1)

1.一种氧化镥透明陶瓷的制备方法，其特征在于：所述的制备方法包括以下步骤：
（1） 将水合硝酸镥2.274g溶于50ml水中，得溶液A；将乙二醇5ml和硫脲1.37g分别加入到溶液A中，磁力搅拌，得均匀混合溶液B，将混合液B置于500℃马弗炉中，燃烧完毕后得到硫氧化镥纳米粉体；水合硝酸镥与硫脲摩尔比为1:3-4，乙二醇与水的体积比为1:10-15；
（2）将步骤(1)所得的硫氧化镥粉体研磨30min，50Mpa双向轴压成型为陶瓷生胚片；将陶瓷生胚片于马弗炉中900-1000℃空气气氛下烧结10-15h，再于真空炉中1400-1500℃烧结2h，最后在马弗炉中900-1000℃空气气氛下退火5-6h，制得氧化镥透明陶瓷。
CN201610536089.2A 2016-07-10 2016-07-10 一种氧化镥透明陶瓷的制备方法 Expired - Fee Related CN106145959B (zh)

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CN100384963C (zh) * 2005-06-28 2008-04-30 中国科学院上海硅酸盐研究所 氧化镥基纳米荧光粉体及其溶液燃烧合成方法
CN100336777C (zh) * 2005-06-28 2007-09-12 中国科学院上海硅酸盐研究所 一种氧化镥基透明陶瓷的制备方法
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CN101333110B (zh) * 2008-07-16 2011-05-04 上海大学 Nd3+离子掺杂的Lu2O3透明激光陶瓷的制备方法
CN102464348A (zh) * 2010-11-18 2012-05-23 中国科学院福建物质结构研究所 一种氧化镥纳米粉体的水热制备方法
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